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Sulfuric acid magnesium salt (1:1) → HCID 178519072, 화합물

HRID 1467667
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HRID 1467667 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.S([O-])([O-])(=O)=O.[Mg+2].[NH2:19][C:20]1[CH:28]=[CH:27][CH:26]=[C:25]2[C:21]=1[CH2:22][O:23][C:24]2=[O:29]>C(#N)C>[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6](/[CH:7]=[N:19]/[C:20]2[CH:28]=[CH:27][CH:26]=[C:25]3[C:21]=2[CH2:22][O:23][C:24]3=[O:29])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 679964-(Trifluoromethyl)benzaldehydeHCID 122846494-Amino-1,3-dihydro-2-benzofuran-1-one

생성물 1

HCID 178519072HCID 178519072, 화합물수율 68.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a stirred mixture of 4-(trifluoromethyl)benzaldehyde (2.8 g, 16.1 mmol) and anhydrous Magnesium sulfate (16 g, 134 mmol) in anhydrous acetonitrile (200 mL) was added 4-aminoisobenzofuran-1(3H)-one (2 g, 13.4 mmol) at room temperature. After the addition, the mixture was stirred at reflux for overnight. The mixture was filtered and the cake was washed with ethyl acetate (50 mL×3). The filtrate was concentrated to give crude product. The crude product was washed with petroleum ether and re-crystallized from ethyl acetate to give the title compound (2.8 g, yield: 68%). LC-MS (ESI) m/z: 306 (M+1)+.

후처리

  1. additionAfter the addition
  2. temperatureat reflux for overnight
  3. filtrationThe mixture was filtered
  4. washthe cake was washed with ethyl acetate (50 mL×3)
  5. concentrationThe filtrate was concentrated
  6. customto give crude product
  7. washThe crude product was washed with petroleum ether
  8. customre-crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-4b000ab114a342978ce3788c075b206c
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999987B2

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